CN114773758A - Vine-like nano composite hydrogel fiber actuator and preparation method and application thereof - Google Patents
Vine-like nano composite hydrogel fiber actuator and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an imitated tendril nano-composite hydrogel fiber actuator as well as a preparation method and application thereof. The composite hydrogel fiber brake is a composite hydrogel fiber formed by photo-initiated free radical polymerization of thermosensitive N-isopropyl acrylamide, N' -methylene bisacrylamide, polyethylene glycol monomethyl ether methacrylate and CNC suspension, and cellulose nanocrystals are embedded in the composite hydrogel fiber to adjust the network density. The composite hydrogel fiber has a radial annular asymmetric network structure, is similar to a cross-sectional structure of a plant vine, has thermal responsiveness, and generates spiral motion similar to the plant vine under thermal stimulation. The preparation method is simple and feasible. The raw materials of the hydrogel fiber actuator have excellent biocompatibility, so the hydrogel fiber actuator has wide application prospect in the fields of artificial intelligence and biomedical materials such as soft robots, artificial muscles, drug controlled release systems, tissue engineering and the like.
Description
Technical Field
The invention relates to a vine-imitated nano-composite hydrogel fiber actuator as well as a preparation method and application thereof, belonging to the technical field of nano-composite hydrogel actuators and preparation thereof.
Background
The soft hydrogel driver is inspired by organisms in the nature, can respond to environmental stimulus to generate shape transformation, and has wide application prospect in the fields of drug delivery, soft robots, tissue engineering and intelligent materials. The shape transition of hydrogels depends fundamentally on the spatial heterogeneity of swelling, and the mismatch in volume changes associated with water absorption/release drives the shape change of the hydrogel. In nature, plant vines naturally form helices to obtain sunlight and niches. This hydration-induced plant movement is due to differences in local swelling behavior, which is mainly determined by the asymmetric microstructure of the dorsal abdominal cells. The whisker cross-sectional area contains a fibrous lignified network gradient from the inner ventral layer to the outer dorsal layer of the helix, which is associated with a change in the porosity density. The higher lignified, more porous dense ventral layer allows for compression and contraction compared to the outer layer, thereby displacing more water, causing the tendrils to bend and then curl. Thus, the plant tendrils can be considered a nanocomposite hydrogel with a gradient of oriented porosity of the fiber network.
To achieve a biomimetic microstructure of the hydrogel actuator, a representative strategy is to introduce nanoparticles that form a cross-linking density gradient through the thickness, thereby enabling the hydrogel actuator to be crimped. However, most of these methods focus on three-dimensional bulk or two-dimensional layered hydrogels, and few involve hydrogel fibers. It has been shown that fibrous drives with twist and twist designs have higher energy densities, can produce greater motion, and can be more generally automated in soft body robots.
Cellulose Nanocrystals (CNC) have stable water dispersibility and hydrophilicity, and are considered to be one of the ideal candidates for network media. Embedding CNC in a hydrogel matrix allows to obtain a continuous structure in a single system. Furthermore, the high aspect ratio avoids physical entanglement, giving uniformly dispersed CNC the ability to support 3D networks. For example, hydrogels inspiring the skin of sea cucumbers have been reported to have CNC as an osmotic network with a flexible-rigid transition under external stimuli, depending on CNC attraction and repulsion interactions. Thus, it is conceivable to use CNC as a medium to tune the asymmetric network of the hydrogel to achieve a reversible dynamic transition.
Disclosure of Invention
The technical problem solved by the invention is as follows: how to obtain a vine-like nanocomposite hydrogel fiber actuator.
In order to solve the technical problem, the invention provides a vine-imitated nano composite hydrogel fiber actuator, which is a composite hydrogel fiber formed by photo-initiated free radical polymerization of N-isopropyl acrylamide, N' -methylene bisacrylamide, polyethylene glycol monomethyl ether methacrylate and cellulose nanocrystalline suspension with the concentration of less than 4 wt%; the composite hydrogel fiber has a radial crescent asymmetric network structure and temperature sensitivity; wherein, the cellulose nanocrystalline is distributed in the gel in a gradient concentration manner and is used for adjusting the network density of the gel.
Preferably, the concentration of the cellulose nanocrystal suspension is 1-3 wt%, and the mass ratios of the N-isopropylacrylamide, the N, N' -methylenebisacrylamide and the polyethylene glycol monomethyl ether methacrylate to the suspension are respectively as follows: 9-10%, 0.13-0.14%, 1.3-1.4%.
The invention also provides a preparation method of the imitated tendril nanocomposite hydrogel fiber actuator, which comprises the following steps:
step 1: firstly, dispersing cellulose nanocrystals in water to prepare a uniform suspension with the concentration of less than 4 wt%; firstly, weighing a certain amount of Cellulose Nanocrystalline (CNC) with the diameter of 20-30nm and the length of 200-300nm, and dispersing the Cellulose Nanocrystalline (CNC) in water to prepare uniform CNC suspension;
and 2, step: adding N-isopropyl acrylamide, N' -methylene bisacrylamide, polyethylene glycol monomethyl ether methacrylate and a photoinitiator in a certain proportion into the suspension obtained in the step 1, and uniformly mixing to prepare a hydrogel fiber precursor liquid;
and step 3: pouring the hydrogel fiber precursor liquid obtained in the step 2 into a fiber mold, standing in a dark condition, and allowing the cellulose nanocrystals in the fiber mold to settle under the action of gravity to form a concentration gradient;
and 4, step 4: and after standing, performing photoinitiated polymerization on the hydrogel fiber precursor liquid in the fiber mold to form hydrogel fibers, thus obtaining the vine-imitated nano composite hydrogel fiber actuator. In the hydrogel fiber forming process, Cellulose Nanocrystals (CNC) are migrated along the tube wall under the flowing action of Marangoni, so that the radial asymmetric structure of the fiber is further promoted, and the cross section of the hydrogel fiber is induced to be in a crescent network structure. The hydrogel fiber has temperature sensitivity, and spiral curling motion similar to plant vines occurs under thermal stimulation.
Preferably, the cellulose nanocrystal in the step 1 has the diameter of 20-30nm and the length of 200-300 nm; the concentration of the cellulose nanocrystals in the suspension is 1-3 wt%.
Preferably, the mass ratios of the N-isopropylacrylamide, the N, N' -methylenebisacrylamide, the polyethylene glycol monomethyl ether methacrylate, and the photoinitiator to the suspension in the step 2 are respectively as follows: 9-10%, 0.13-0.14%, 1.3-1.4%, 0.18-0.22%; the photoinitiator is alpha, alpha-diethoxyacetophenone.
Preferably, the standing time in the step 3 is more than or equal to 8 h.
Preferably, the conditions for photoinitiated polymerization in the step 4 are as follows: initiating polymerization under 365nm ultraviolet lamp illumination, wherein the illumination density is 0.32mW cm-2The illumination time is 20-60 min.
The invention also provides the vine-imitated nano-composite hydrogel fiber actuator, and the application of the vine-imitated nano-composite hydrogel fiber actuator prepared by the preparation method in artificial intelligence materials and biomedical materials.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the vine-imitated nano composite hydrogel fiber actuator, the height of a fiber network structure is consistent with that of a network structure in a plant vine, and due to the radial annular crescent network structure, spiral motion can be generated under thermal stimulation, so that the bionic from a microstructure to a macroscopic property is realized;
(2) the hydrogel fiber prepared by the invention has thermal responsiveness, generates spiral motion similar to plant vines under thermal stimulation, has the fastest response speed of 15s and the energy density of 28.39kJ m-3；
(3) The poly-N-isopropylacrylamide, the N, N' -methylenebisacrylamide, the polyethylene glycol monoethyl ether methacrylate and the cellulose nanocrystal in the hydrogel fiber actuator prepared by the invention have excellent biocompatibility and do not form any stimulation to skin, tissues, eyes and the like, so the hydrogel fiber actuator has wide application prospect in the fields of artificial intelligence and biomedical materials such as soft robots, artificial muscles, drug controlled release systems, tissue engineering and the like;
(4) the preparation method of the vine-imitated nano composite hydrogel fiber actuator provided by the invention does not need to use a complex external field, is simple and feasible in process, realizes the asymmetric structure forming in a single hydrogel fiber in a one-step polymerization process, and avoids complex multilayer structure design.
Drawings
Fig. 1 is a molecular formula of raw materials for the vine-like nanocomposite hydrogel fiber actuator of the invention, which comprises: cellulose Nanocrystals (CNC), N-isopropylacrylamide (NIPAM), N' -methylenebisacrylamide (bis), polyethylene glycol monoethyl ether methacrylate (PEGMEMA) and photoinitiator alpha, alpha-Diethoxyacetophenone (DEAP);
fig. 2 is a process for designing and manufacturing the vine-like nanocomposite hydrogel fiber actuator of the present invention, wherein a is a spiral vine photo, b is a schematic diagram of a vine side cut surface network structure showing different network densities on the inner and outer sides, c is a process for manufacturing the vine-like nanocomposite hydrogel fiber actuator, and d is a motion state of the fiber section nanoparticles during the preparation of the vine-like nanocomposite hydrogel fiber actuator;
FIG. 3 is a graph showing the flow of gel in the axial direction of the fiber due to Marangoni effect during the preparation of the vine-like nanocomposite hydrogel fiber actuator according to the present invention;
fig. 4 is a distribution and network structure of nanoparticles in a fiber section of the vine-like nanocomposite hydrogel fiber actuator according to the present invention, wherein a is a three-dimensional confocal imaging diagram of fluorescently labeled nanoparticles on the fiber section, b is a fiber section dyed by methylene blue, wherein a region with a large CNC distribution is dark in color due to the network being tight and not prone to dye intrusion, C is a SEM diagram of the vine-like nanocomposite hydrogel fiber section, d is a distribution of elements at the Top (Top) and Bottom (Bottom) on the fiber section corresponding to the diagram C, and the content of the Bottom C is increased, which indicates that the nanoparticles are distributed more at the Bottom;
FIG. 5 is a photograph showing that the vine-like nanocomposite hydrogel fiber actuator prepared in example 1 responds to a screw motion in hot water at 60 ℃, and the screw motion is completed within 15 s;
FIG. 6 is a photograph of the simulated spiral climbing motion of the simulated tendril nanocomposite hydrogel fiber actuator prepared in example 1, which completes the spiral climbing within 18s and successfully climbs to the support;
FIG. 7 is a graph showing response curves of the simulated tendril nanocomposite hydrogel fiber actuators prepared in examples 1-3 (with different CNC contents) at 60 ℃ and a comparison of response rates at different temperatures;
FIG. 8 is a photograph (a) showing the distribution of nanoparticles in a fiber section of a nanocomposite hydrogel prepared in comparative example and (b) showing no spiral motion in hot water at 60 ℃.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
In the following examples, cellulose nanocrystals (diameter 20-30nm, length 200-300nm) were obtained from the Karsch technology (Science K), N-isopropylacrylamide (98%) was obtained from TCI Chiese (Shanghai) chemical industry Co., Ltd., N' -methylenebisacrylamide (99%), polyethylene glycol monomethyl ether methacrylate (M)n＝500g mol-1) And photoinitiator alpha, alpha-diethoxyacetophenone was purchased from alatin reagent (shanghai) ltd.
The test procedures and conditions for the performance data in the following examples are as follows: observing a flow chart and a fiber section dyeing chart in the forming process of the plant vines and the fibers by using a microscope (Nikon Eclipse Ni-U, a fluorescence mode and a bright field mode); the fiber section particle distribution diagram is tested by a laser confocal microscope (come card TCS SP5II, 405nm, single channel), before the test, the fiber is cut into slices with the diameter of not more than 0.5mm along the radial direction, and the slices are soaked in water to prevent water evaporation and structural damage; observing the appearance of the fiber by using a field emission scanning electron microscope (Hitachi, SU8000, 3kV of voltage), soaking the hydrogel fiber in liquid nitrogen for freezing and brittle fracture before testing, keeping the cross-sectional structure of the fiber, then placing the frozen fiber in a freeze dryer for drying, taking out after 1 day, and spraying gold on the surface of a sample for 30s to increase the conductivity; the actuation process of the vine-imitated nanocomposite hydrogel fiber actuator was recorded using a Canon EOS 80D camera, and before testing, the fiber was cut into 5cm long samples and soaked in water.
Example 1
A preparation method of an imitated tendril nanocomposite hydrogel fiber actuator comprises the following steps:
dispersing 0.02g CNC into 2mL deionized water, stirring thoroughly, performing ultrasonic treatment for 10s in ice bath by using a cell crusher, adding 0.2g N-isopropyl acrylamide (NIPAM) and 0.0027g N, N' -methylene into the suspensionBisacrylamide (bis), 27. mu.L of polyethylene glycol monomethyl ether methacrylate (PEGMEMA), 4. mu.L of photoinitiator DEAP, stirred at room temperature in the dark for 30 min. And (3) pouring the hydrogel precursor solution into a 1.5mm fiber mould, horizontally standing in a dark environment, and standing at room temperature for 8 hours. Placing the hydrogel fiber precursor in ultraviolet light (365nm, 0.32mW cm)-2) And initiating for 20min to polymerize to obtain the nanometer composite hydrogel fiber. Standing and aging the fiber at room temperature for 12h, taking the fiber out of a mold, and fully soaking the fiber in deionized water for 48 h. The prepared nano composite hydrogel fiber has a crescent asymmetric network structure, and the response time of spiral motion at 60 ℃ is 15 s.
Example 2
A preparation method of an imitated tendril nanocomposite hydrogel fiber actuator comprises the following steps:
0.04g of CNC is dispersed into 2mL of deionized water, the mixture is fully stirred, ultrasonic treatment is carried out for 10s under ice bath by using a cell crusher, 0.2g N-isopropyl acrylamide (NIPAM), 0.0027g of N, N' -methylene-bis-acrylamide (bis), 27 mu L of polyethylene glycol monomethyl ether methacrylate (PEGMEMA) and 4 mu L of photoinitiator DEAP are added into the suspension, and the mixture is stirred for 30min at room temperature in a dark place. And (3) pouring the hydrogel precursor solution into a 1.5mm fiber mould, horizontally standing in a dark environment, and keeping the temperature at room temperature for 8 hours. Placing the hydrogel fiber precursor in ultraviolet light (365nm, 0.32mW cm)-2) And initiating for 20min to polymerize to obtain the nanometer composite hydrogel fiber. And standing and aging the fiber at room temperature for 12h, taking the fiber out of the mold, and fully soaking the fiber in deionized water for 48 h. The prepared nano composite hydrogel fiber has a crescent asymmetric network structure, and the response time of spiral motion at 60 ℃ is 20 s.
Example 3
A preparation method of an imitated tendril nanocomposite hydrogel fiber actuator comprises the following steps:
dispersing 0.06g CNC into 2mL deionized water, stirring thoroughly, performing ultrasonic treatment for 10s in ice bath by using a cell crusher, adding 0.2g N-isopropyl acrylamide (NIPAM), 0.0027g N, N' -methylene-bisacrylamide (bis), 27 μ L polyethylene glycol monomethyl ether methacrylate (PEGMEMA) into the suspension,mu.L of photoinitiator DEAP is stirred for 30min at room temperature in the dark. And (3) pouring the hydrogel precursor solution into a 1.5mm fiber mould, horizontally standing in a dark environment, and standing at room temperature for 8 hours. Placing the hydrogel fiber precursor in ultraviolet light (365nm, 0.32mW cm)-2) And initiating for 20min to polymerize to obtain the nanometer composite hydrogel fiber. Standing and aging the fiber at room temperature for 12h, taking the fiber out of a mold, and fully soaking the fiber in deionized water for 48 h. The prepared nano composite hydrogel fiber has a crescent asymmetric network structure, and the response time of spiral motion at 60 ℃ is 15 s; by the formula: energy density of Qout/Vfiber，Qout＝χ(△x)2Calculated fiber energy density of 28.39kJ m-3Wherein chi is the elastic coefficient of the fiber and is obtained through a stress-strain curve of the fiber; Δ x is the distance of fiber movement within 15 s; vfiberIs the fiber volume.
And (3) performance testing:
inspired by the spiral climbing growth behavior (such as cucumber tendrils) in the growth process of plant fibers, ferroferric oxide magnetic particles are adsorbed at one end of the nano-composite hydrogel fiber prepared in the example 1, so that the nano-composite hydrogel fiber has magnetism. The fiber is placed in hot water at 60 ℃, the magnet is adopted to attract the fiber end with the magnetic particles to help the fiber end to find the attachment, then the magnet is removed, the hydrogel fiber can be automatically wound along the attachment, and the bionic from the structure to the function is realized.
Figure 6 shows the biomimetic spiral climbing behavior of the nanocomposite hydrogel fibers within 18 s.
Comparative example
Dispersing 0.08g of CNC into 2mL of deionized water, fully stirring, performing ultrasonic treatment for 10s in ice bath by using a cell crusher, adding 0.2g N-isopropylacrylamide (NIPAM), 0.0027g of N, N' -methylenebisacrylamide (bis), 27 mu L of polyethylene glycol monomethyl ether methacrylate (PEGMEMA) and 4 mu L of photoinitiator DEAP into the suspension, and stirring for 30min at room temperature in a dark place. And (3) pouring the hydrogel precursor solution into a 1.5mm fiber mould, horizontally standing in a dark environment, and keeping the temperature at room temperature for 8 hours. Placing the hydrogel fiber precursor in ultraviolet light (365nm, 0.32mW cm)-2) Lower partAnd initiating polymerization for 20min to obtain the nano composite hydrogel fiber. Standing and aging the fiber at room temperature for 12h, taking the fiber out of a mold, and fully soaking the fiber in deionized water for 48 h. Because the CNC concentration is too high, the viscosity of the CNC suspension is sharply increased, the CNC cannot be settled by gravity, and the prepared nano-composite hydrogel fiber does not have a crescent asymmetric network structure and does not generate spiral motion at 60 ℃.
FIG. 8a shows that the nano-composite hydrogel fiber prepared as above has uniformly distributed nanoparticles in the cross-section, thus having no asymmetric network structure, and does not have spiral motion at 60 deg.C (1min), as shown in FIG. 8 b.
Claims (8)
1. A vine-imitated nano composite hydrogel fiber actuator is characterized in that composite hydrogel fibers are formed by photo-initiated free radical polymerization of N-isopropyl acrylamide, N' -methylene bisacrylamide, polyethylene glycol monomethyl ether methacrylate and cellulose nanocrystalline suspension with the concentration of less than 4 wt%; the composite hydrogel fiber has a radial crescent asymmetric network structure and temperature sensitivity; wherein, the cellulose nanocrystalline is distributed in the gel in a gradient concentration manner and is used for adjusting the network density of the gel.
2. The cranberry-like nanocomposite hydrogel fiber actuator of claim 1, wherein the cellulose nanocrystal suspension has a concentration of 1-3 wt%, and the mass ratios of the N-isopropylacrylamide, the N, N' -methylenebisacrylamide, and the polyethylene glycol monomethyl ether methacrylate to the suspension are: 9-10%, 0.13-0.14%, 1.3-1.4%.
3. The method of making an cranberry-like nanocomposite hydrogel fiber actuator of claim 1, comprising the steps of:
step 1: firstly, dispersing cellulose nanocrystals in water to prepare a uniform suspension with the concentration of less than 4 wt%;
step 2: adding N-isopropyl acrylamide, N' -methylene bisacrylamide, polyethylene glycol monomethyl ether methacrylate and a photoinitiator in a certain proportion into the suspension obtained in the step 1, and uniformly mixing to prepare a hydrogel fiber precursor liquid;
and 3, step 3: pouring the hydrogel fiber precursor liquid obtained in the step (2) into a fiber mold, standing in a dark condition, and allowing the cellulose nanocrystals in the fiber mold to settle under the action of gravity to form a concentration gradient;
and 4, step 4: and after standing, carrying out photoinitiated polymerization on the hydrogel fiber precursor liquid in the fiber mold to form hydrogel fibers, thus obtaining the vine-imitated nano composite hydrogel fiber actuator.
4. The method for preparing the vine-like nanocomposite hydrogel fiber actuator as claimed in claim 3, wherein the cellulose nanocrystals obtained in step 1 have a diameter of 20-30nm and a length of 200-300 nm; the concentration of the cellulose nanocrystals in the suspension is 1-3 wt%.
5. The method for preparing the vine-like nanocomposite hydrogel fiber actuator as claimed in claim 3, wherein the mass ratios of the N-isopropylacrylamide, the N, N' -methylenebisacrylamide, the polyethylene glycol monomethyl ether methacrylate and the photoinitiator to the suspension in the step 2 are respectively as follows: 9-10%, 0.13-0.14%, 1.3-1.4%, 0.18-0.22%; the photoinitiator is alpha, alpha-diethoxyacetophenone.
6. The preparation method of the vine-like nanocomposite hydrogel fiber actuator as claimed in claim 3, wherein the standing time in step 3 is not less than 8 h.
7. The method of making an anfrac-like nanocomposite hydrogel fiber actuator of claim 3, wherein the conditions of the photo-initiated polymerization in step 4 are: initiating polymerization under 365nm ultraviolet lamp illumination, wherein the illumination density is 0.32mW cm-2The illumination time is 20-60 min.
8. The use of the vine-like nanocomposite hydrogel fiber actuator as claimed in claim 1 or 2, or the use of the vine-like nanocomposite hydrogel fiber actuator prepared by the preparation method as claimed in any one of claims 2 to 7 in artificial intelligence materials and biomedical materials.
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